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Near-Real Time Measurement of Carbonaceous Aerosol Using Microplasma Spectroscopy: Application to Measurement of Carbon Nanomaterials

机译:微等离子体光谱法近距离测量碳质气​​溶胶:在碳纳米材料测量中的应用

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摘要

A sensitive, field-portable microplasma spectroscopy method has been developed for real-time measurement of carbon nanomaterials. The method involves microconcentration of aerosol on a microelectrode tip for subsequent analysis for atomic carbon using laser-induced breakdown spectroscopy (LIBS) or spark emission spectroscopy (SES). The spark-induced microplasma was characterized by measuring the excitation temperature (15,000 – 35,000 K), electron density (1.0 × 1017 – 2.2 × 1017 cm−3), and spectral responses as functions of time and interelectrode distance. The system was calibrated and detection limits were determined for total atomic carbon (TAC) using a carbon emission line at 247.856 nm (C I) for various carbonaceous materials including sucrose, EDTA, caffeine, sodium carbonate, carbon black, and carbon nanotubes. The limit of detection for total atomic carbon was 1.61 ng, equivalent to 238 ng m−3 when sampling at 1.5 L min−1 for 5 min. To improve the selectivity for carbon nanomaterials, which consist of elemental carbon (EC), the cathode was heated to 300 °C to reduce the contribution of organic carbon to the total atomic carbon. Measurements of carbon nanotube aerosol at elevated electrode temperature showed improved selectivity to elemental carbon and compared well with the measurements from thermal optical method (NIOSH Method 5040). The study shows that the SES method to be an excellent candidate for development as a low-cost, hand-portable, real-time instrument for measurement of carbonaceous aerosols and nanomaterials.
机译:已经开发出一种灵敏的,便携式的等离子光谱技术,用于实时测量碳纳米材料。该方法包括在微电极尖端上对气溶胶进行微量浓缩,以便随后使用激光诱导击穿光谱法(LIBS)或火花发射光谱法(SES)对原子碳进行分析。通过测量激发温度(15,000 – 35,000 K),电子密度(1.0×10 17 – 2.2×10 17 cm -)来表征火花诱导的微等离子体3 ),光谱响应随时间和电极间距离而变化。对该系统进行了校准,并使用247.856 nm(C I)处的碳发射线测定了包括蔗糖,EDTA,咖啡因,碳酸钠,碳黑和碳纳米管在内的各种碳质材料的总原子碳(TAC)的检出限。在1.5 L min -1 采样5分钟时,总原子碳的检出限为1.61 ng,相当于238 ng m -3 。为了提高由元素碳(EC)组成的碳纳米材料的选择性,将阴极加热到300°C,以减少有机碳对总原子碳的贡献。在升高的电极温度下对碳纳米管气溶胶的测量显示出对元素碳的选择性提高,并且与热光学方法(NIOSH方法5040)的测量结果进行了很好的比较。研究表明,SES方法是开发低成本,便携式,实时测量碳质气​​溶胶和纳米材料的理想选择。

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